反应详情

6-Chloropyrid-3-ylcarbonyl chloride (0.37 g) was added to a mixture of N-(3-amino4-methylphenyl)-3-dimethylaminobenzamide (0.54 g), potassium carbonate (0.304 g), DMF (5 ml) and methylene chloride (20 ml) and the resultant mixture was stirred at ambient temperature for 16 hours. The mixture was poured into water and extracted with ethyl acetate. The organic extracts were washed with a saturated aqueous sodium chloride solution, dried over magnesium sulphate and evaporated. The residue was purified by column chromatography on silica using a 3:2:1 mixture of isohexane, ethyl acetate and methylene chloride as eluent. There was thus obtained the title compound as a solid (0.122 g); NMR Spectrum: (DMSOd6) 2.19 (s, 6H), 3.28 (s, 3H), 6.88 (m, 1H), 7.25 (m, 4H), 7.57 (m, 1H), 7.7 (d, 1H), 7.84 (d, 1H), 8.36 (m, 1H), 8.95 (d,1H), 10.11 (s, 1H), 10.16 (s, 1H); Mass Spectrum: M+H+ 409 and 411.

1. extractionextracted with ethyl acetate
2. washThe organic extracts were washed with a saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. customevaporated
5. customThe residue was purified by column chromatography on silica using
6. additiona 3:2:1 mixture of isohexane, ethyl acetate and methylene chloride as eluent